CN104557013B - Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics - Google Patents
Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics Download PDFInfo
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Abstract
The invention relates to a preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics. The preparation method comprises the following steps: weighing raw material powder according to a stoichiometric ratio of a to-be-prepared ceramic component structural formula (Al1-xCrx)5CayY3-yO12 (x is not smaller than 0.001 and not larger than 0.01, and y is not smaller than 10x and not larger than 40x); adding a sintering aid and a charge compensating agent; mixing by ball-milling to obtain a slurry material; drying and sieving the slurry material and then molding to obtain a biscuit; calcining to remove volatile impurities; sintering the biscuit in vacuum at the temperature of 1730 to 1850 DEG C for 4 to 30 hours; subsequently annealing in air at the temperature of 1300 to 1550 DEG C for 10 to 25 hours to obtain compact Cr＜4+＞:YAG transparent ceramics. The Cr＜4+＞:YAG transparent ceramics prepared by the method disclosed by the invention are high in compactness, good in uniformity, free of segregation, reasonable in grain graduation distribution, free of abnormal grain growth, free of grain interior and intergranular pores and high in penetration rate, and have the conditions for being a laser gain medium.
Description
Technical field
The present invention relates to a kind of preparation method of tetravalence chromium dopping yttrium aluminum garnet transparent ceramic, more particularly to one
Plant with tetraethyl orthosilicate (TEOS), B2O3And CaCO3For auxiliary agent is prepared with superior optical quality and tetravalence chromium conversion ratio high
Cr4+:YAG crystalline ceramics, belongs to advanced ceramics preparation field.
Background technology
1964, Shkadarevich etc. was prepared for tetravalence chromium doping YAG monocrystalline using czochralski method first, and by widely
As tunable laser gain media.With the gain media (Cr for being conventionally used to tunable laser4+:Mg2O4,Ti3+:Al2O3
Deng) compare, Cr4+:YAG monocrystalline has quantum efficiency high, good stability and with advantages such as fluorescence lifetimes more long.Not only such as
This, because tetravalence chromium ion has saturable absorption characteristic in 1000nm~1200nm, can not only as saturable absorber,
With Nd3+And Yb3+Realize that passively Q switched laser is exported, it is also possible to for suppressing parasitic concussion effect, in scientific research, military affairs, medical treatment etc.
There is quite varied application in various fields.
Although czochralski method single crystal preparation technique have passed through the development of many decades, people have been overcome in many preparation technologies
Defect, but still there are many problems cannot still to efficiently solve so far, the such as production cycle is long, energy consumption is big, optics is equal
Even property is poor, be difficult to high-concentration dopant etc., significantly limit its development.For a long time, people always search for substituting material
Material, until nineteen ninety-five, Japanese Scientists A.Ikesue is prepared for high-quality Nd using solid phase reaction sintering process:YAG crystalline ceramics,
And the continuous laser output of 1064nm is realized first.Compared with monocrystal material, transparent laser ceramic is with its short preparation period, production
Low cost, optical homogeneity are good, easily controllable shape and size and to be easily achieved multi-layer structure design and multifunction etc. excellent
Gesture, development is very rapid, and at present, various rare earth ion doped laser transparent ceramic materials emerge in an endless stream, such as YAG, times semi-oxidized
The systems such as thing, spinelle, fluoride, various ceramic base laser outputs are also reported in succession, and in many key areas
Preliminary Applications are obtained, its substitution monocrystalline turns into gain medium of future generation and just progressively becomes a reality, and development prospect is very wide.
In all of transparent ceramic material system, YAG base transparent ceramics, with its excellent material property, are laser material research fields
Focus and emphasis, the transparent ceramic material system that achievement in research is the plentifulest and substantial, be most widely used is had become at present.
Although the research of current people YAG transparent ceramic materials La rear earth ion doped to trivalent has been achieved for plentiful and substantial
Achievement, but so far, on possess superior optical quality tetravalence chromium doping YAG crystalline ceramics report but seldom,
Because La rear earth ion doped different from trivalent, the introducing of tetravalence chromium will necessarily cause charge imbalance (Cr4+=Cr3++
e-), the case of the trivalent aluminium ion being difficult under normal circumstances in substitution YAG lattices, in order to make up this defect, it usually needs draw
Enter divalent charge counterion into generation Lacking oxygen in YAG lattices to capture the electronics produced when tetravalence chromium is formed, so that real
Existing charge balance.It is also well known that TEOS is typically used as the sintering aid of YAG crystalline ceramics, because TEOS can be heated
Resolve into SiO2, according to YAG-SiO2Phasor, YAG meetings and SiO at about 1400 DEG C2Generation liquid phase, makes flooding mechanism by solid phase
Diffusion transformation is spread for liquid phase, greatly lifts diffusion rate, therefore, it is possible to promote YAG potteries while sintering temperature is reduced
The densification of porcelain, contributes to improving optical quality.But and Cr4+Equally, Si4+Aluminum ions lattice in YAG lattices can equally be replaced
Position, in addition Si4+Electronegativity be far above Cr4+, therefore Charge-compensating ions can preferentially balance Si4+The charge imbalance for being brought, pole
The earth inhibits the conversion ratio of tetravalence chromium, therefore is preparing Cr:YAG crystalline ceramics is the addition for needing to consider carefully TEOS,
To balance Cr4+:The optical quality of YAG crystalline ceramics and the conversion ratio of tetravalence chromium.
In Cr4+:The preparation aspect of YAG crystalline ceramics, document 1 (A.Ikesue, K.Yoshida, K.Kamata,
J.Am.Ceram.Soc., 79 (1996) 507-509.) using the high pure oxide raw material of laboratory synthesis, CaCO3Used with MgO
Make charge compensation, 0.5wt%TEOS is sintered and vacuum-sintering+oxygen atmosphere annealing by oxygen atmosphere respectively as sintering aid
Both techniques are prepared for 0.1at%Cr:YAG crystalline ceramics, the Cr that final oxygen atmosphere is fired:The baseline of YAG crystalline ceramics
Transmitance only has 70%, and the baseline transmitance of the sample of vacuum-sintering+oxygen atmosphere annealing also only has 80%, and completely without real
Existing tetravalence chromium conversion.Document 2 (J.Li, W.Liu, B.Jiang, J.Zhou, et.al, J.Alloy.Compd., 515 (2012)
High-purity commercial oxidation powder raw material 49-56.) is used, appropriate CaO and TEOS is auxiliary agent, is followed by through 1780 DEG C of vacuum-sintering 10h
The 20h that annealed in 1450 DEG C of air, 0.1at.%Cr, 1.0at.%Nd is prepared for:YAG crystalline ceramics, but transmitance and four
Valency chromium conversion situation is little with the difference of document 1.Document 3 (W.Liu, J.Li, J.Liu, et.al, Ceram.Int., 40 (2014)
8879-8883.) using the preparation technology of document 2, the addition of CaO and TEOS is optimized, although the 0.1at%Cr for preparing:
YAG crystalline ceramics baselines transmitance reaches 83%, but tetravalence chromium conversion ratio is still very low.
In the Cr that document above is reported4+:YAG crystalline ceramics generally existings that tetravalence chromium conversion ratio is relatively low or transmitance
Relatively low the problems such as, it is far from reaching Cr4+:The optical quality of YAG monocrystalline, it is impossible to main former for realizing laser output or adjusting Q
Because being exactly not select suitable sintering aid system.
The content of the invention
It is an object of the invention to provide a kind of tetravalence chromium doped yttrium aluminum garnet in order to improve the deficiencies in the prior art
The preparation method of crystalline ceramics, the method with high-purity commercial oxidation powder as raw material, CaCO3As charge compensator, TEOS
And B2O3The Cr with excellent transmitance and tetravalence chromium conversion ratio higher is prepared for sintering aid4+:YAG crystalline ceramics.
The technical scheme is that：A kind of tetravalence chromium doped yttrium aluminum garnet (Y3Al5O12, YAG) crystalline ceramics system
Preparation Method, it is characterized in that prepared ceramic composition meets following formula:
(Al1-xCrx)5CayY3-yO12
The scope of x takes 0.001≤x≤0.01 in formula, and the scope of y takes 10x≤y≤40x and comprises the following steps that：
(1) dispensing and ball milling：Material powder Al is weighed by the stoichiometric proportion of required metallic element2O3、Y2O3And Cr2O3
Powder, and add sintering aid and charge compensator CaCO3Carry out dispensing；Institute is obtained after ball milling mixing on planetary ball mill
Use slurry；
(2) it is molded：By the slurry drying obtained by step (1), sieving after be placed in it is dry-pressing formed in mould, then through supercooling
Isostatic pressing obtains biscuit, calcines to remove volatile impurity；
(3) sinter and anneal：Biscuit obtained by step (2) is used into 1730 DEG C~1850 DEG C 4~30h of vacuum-sintering,
Then 10~the 25h that annealed in 1300 DEG C~1550 DEG C is placed in air, fine and close Cr is obtained final product4+:YAG crystalline ceramics.
Raw material is chosen：Al raw materials are from commercially available high-purity (99.99% and more than) Al2O3Powder；Y, Cr raw material select commercially available height
Pure (99.99% and more than) Y2O3And Cr2O3Powder；CaCO3As charge compensator, tetraethyl orthosilicate (TEOS) and B2O3
(99.99% and more than) is used as the co-sintering auxiliary agent of crystalline ceramics；
It is preferred that described sintering aid is tetraethyl orthosilicate and B2O3The co-sintering auxiliary agent of composition；Wherein B2O3Mole
It is 2~8 times of Cr ion atoms percentage in ceramic composition；TEOS consumptions are respectively the 0.05~0.50% of gained YAG mass.
Drum's speed of rotation is 120~300r/min in preferred steps (1)；Ball-milling Time is 8~18 hours.
The pressure of cold isostatic compaction is 150~250MPa in preferred steps (2)；Calcining heat is 800 DEG C~1000 DEG C,
Calcination time is 5~10h.
Beneficial effect：
1. Cr prepared by the method for being provided with the present invention4+:YAG crystalline ceramics consistency is high, uniformity is good, segregation-free, brilliant
Grade with being reasonably distributed, grow up, and without transgranular and intergranular stomata, transmitance is high by crystal grain without exception, possesses and is situated between as laser gain
The condition of matter.
2. Cr prepared by the method for being provided with the present invention4+:The technological process of YAG crystalline ceramics is simple, by the excellent of auxiliary agent
Change, tetravalence chromium conversion ratio higher can be obtained on the premise of transmitance is not influenceed, be highly suitable for as saturable absorption
Body realizes that passively Q switched laser is exported.
Brief description of the drawings
Fig. 1：According to Cr prepared by example 14+:Polished surface (a) and section (b) the SEM figure of YAG
Fig. 2：According to Cr prepared by example 24+:Polished surface (a) and section (b) the SEM figure of YAG
Fig. 3：According to Cr prepared by example 34+:Polished surface (a) and section (b) the SEM figure of YAG
Fig. 4：According to Cr prepared by example 1,2,34+:The XRD spectrum (respectively a, b, c) of YAG, is pure YAG phases；
Fig. 5：It is the Cr prepared according to example 14+:The transmittance curve of YAG, shows the ceramics while having transmission higher
Rate and tetravalence chromium conversion ratio.
Specific embodiment
(n represents B in table for specific embodiment component of the invention such as table 12O3Molal quantity)：
Table 1
Embodiment 1#：
1 in composition such as table 1#Shown, specific preparation method comprises the following steps：
1. the composition pressed in table 1 weighs raw material, and oxide raw material powder is put into high purity aluminium oxide ball grinder first, plus
Enter sintering aid, charge balance agent, absolute ethyl alcohol configuration slurry；Ball milling mixing 10 hours on planetary ball mill, rotating speed is
160r/min, obtains preparing Cr4+:YAG crystalline ceramics slurry therewiths；
2. step 1. in the slurry that obtains be placed in 55 DEG C of baking ovens and dry and sieve, then by resulting powder mould
Disk is pressed into 60Mpa dry-pressing, then biscuit is obtained by 200MPa isostatic cool pressings.
3. by step 2. gained biscuit 920 DEG C of biscuiting 8h in air, then 1780 DEG C of vacuum-sintering 8h, last 1500 are placed in
The 15h that annealed in DEG C air obtains final product fine and close Cr4+:YAG crystalline ceramics, after ground, polishing, the polished surface and section of ceramics sample
SEM figures are shown in Fig. 1, show that the ceramics have complete densified structure, and the XRD spectrum of sample is shown in Fig. 4, is pure YAG phases, sample
Transmittance curve (Lambda950, Perkin elmer) is shown in Fig. 5, and its straight line transmittance at 2000nm is 85.07%,
There is obviously tetravalence chromium absworption peak at 1030nm, show the high conversion rate of tetravalence chromium.
Embodiment 2#：
2 in composition such as table 1#Shown, specific preparation method comprises the following steps：
1. the composition pressed in table 1 weighs raw material, and oxide raw material powder is put into high purity aluminium oxide ball grinder first, and
Add sintering aid, charge balance agent, absolute ethyl alcohol configuration slurry；Ball milling mixing 18 hours, rotating speed on planetary ball mill
It is 120r/min, obtains preparing Cr4+:YAG crystalline ceramics slurry therewiths；
2. step 1. in the slurry that obtains dried according to step technological parameter 2. in embodiment 1, sieved, dry-pressing,
Then biscuit is obtained in 150Mpa isostatic cool pressings.
4. by step 2. gained biscuit 800 DEG C of biscuiting 10h in air, then 1730 DEG C of vacuum-sintering 30h are placed in, finally
The 25h that annealed in 1300 DEG C of air obtains final product fine and close Cr4+:YAG crystalline ceramics, after ground, polishing, the throwing of ceramics sample ceramics sample
Optical surface and section SEM figures are shown in Fig. 2, show that the ceramics have complete densified structure, and the XRD spectrum of sample is shown in Fig. 4, is
Pure YAG phases, straight line transmittance of the sample at 2000nm is 84.56%, has obviously tetravalence chromium to absorb at 1030nm
Peak.
Embodiment 3#：
3 in composition such as table 1#Shown, specific preparation method comprises the following steps：
1. the composition pressed in table 1 weighs raw material, and oxide raw material powder is put into high purity aluminium oxide ball grinder first, plus
Enter sintering aid, charge balance agent, absolute ethyl alcohol configuration slurry；Ball milling mixing 8 hours on planetary ball mill, rotating speed is
300r/min, obtains preparing Cr4+:YAG crystalline ceramics slurry therewiths；
2. step 1. in the slurry that obtains dried according to step technological parameter 2. in embodiment 1, sieved, dry-pressing,
Then biscuit is obtained in 250Mpa isostatic cool pressings.
4. by step 2. gained biscuit 1000 DEG C of biscuiting 5h in air, then 1850 DEG C of vacuum-sintering 4h are placed in, finally
The 10h that annealed in 1550 DEG C of air obtains final product fine and close Cr4+:YAG crystalline ceramics, after ground, polishing, the throwing of ceramics sample ceramics sample
Optical surface and section SEM figures are shown in Fig. 3, show that the ceramics have complete densified structure, and the XRD spectrum of sample is shown in Fig. 4, is
Pure YAG phases, straight line transmittance of the sample at 2000nm is 83.29%, has obviously tetravalence chromium to absorb at 1030nm
Peak.
Claims (3)
1. a kind of preparation method of tetravalence chromium dopping yttrium aluminum garnet transparent ceramic, it is characterized in that prepared ceramic composition meets
Following formula：
(Al1-xCrx)5CayY3-yO12
The scope of x takes 0.001≤x≤0.01 in formula, and the scope of y takes 10x≤y≤40x；Comprise the following steps that：
(1) dispensing and ball milling：Material powder Al is weighed by the stoichiometric proportion of required metallic element2O3、Y2O3And Cr2O3Powder
Body, and add sintering aid and charge compensator CaCO3Carry out dispensing；Obtain used after ball milling mixing on planetary ball mill
Slurry；Wherein described sintering aid is tetraethyl orthosilicate and B2O3The co-sintering auxiliary agent of composition, B2O3Mole be ceramic group
2~8 times of Cr ion atoms percentages in point, TEOS consumptions are respectively the 0.05~0.50% of gained YAG mass；
(2) it is molded：By the slurry drying obtained by step (1), sieving after be placed in it is dry-pressing formed in mould, then through supercooling etc. it is quiet
It is molded to obtain biscuit, calcine to remove volatile impurity；
(3) sinter and anneal：Biscuit obtained by step (2) is used into 1730 DEG C~1850 DEG C 4~30h of vacuum-sintering, then
10~the 25h that annealed in 1300 DEG C~1550 DEG C is placed in air, fine and close Cr is obtained final product4+:YAG crystalline ceramics.
2. the preparation method as described in claim 1, it is characterised in that drum's speed of rotation is 120~300r/min in step (1)；
Ball-milling Time is 8~18 hours.
3. the preparation method as described in claim 1, it is characterised in that in step (2) pressure of cold isostatic compaction be 150~
250MPa；Calcining heat is 800 DEG C~1000 DEG C, and calcination time is 5~10h.
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| CN107129293A (en) * | 2017-06-08 | 2017-09-05 | 江苏师范大学 | A kind of preparation method of Mg adjuvant systems YAG base transparent ceramics |
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| CN108947516B (en) * | 2018-08-29 | 2021-04-06 | 江苏师范大学 | (Cu, Ce): YAG transparent fluorescent ceramic and preparation method and application thereof |
| US11225439B2 (en) * | 2019-02-12 | 2022-01-18 | Jx Nippon Mining & Metals Corporation | Cr:YAG sintered body and production method thereof |
| CN112209710A (en) * | 2020-10-17 | 2021-01-12 | 江苏师范大学 | Method for preparing Ce: YAG fluorescent ceramic by laser sintering |
| CN114920548B (en) * | 2022-03-16 | 2023-05-16 | 江苏师范大学 | Flash firing Cr preparation 3+ Method for doping garnet-based transparent ceramics |
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